Process for treating mineral oils



April 14, 1936. M. R. FENSKEY. ET AL 2,037,319

PROCESS FOR TREATING MINERAL OILS Filed NOV. 21, 1953. 5 Sheets-Sheet l game/M1044 April 14, M R FENSKE AL PROCESS FOR TREATING MINERAL OILS v Filed Nov. 21; 1953 s Sheets-Sheet 2 April 14, 1936. M. R. FENSKE ET AL 2,037,319

PROCESS FOR TREATING MINERAL OILS v I Filed N v. 21, 1933 5 Sheets-Sheet 3 a7 80 [79 m 78 mi iiii mm n; m! in I iiil m l 1 M! n mI H-i. 98 4/2 2 I P lT/I I XII/l .93 in m April 14, 1936. M. R. FENSKE ET AL PROCESS FOR TREATING MINERAL OILS Filed Nov. 21, 1955 5 Sheets-Sheet 4 3mm Alerrellfll'emk *vifilbenbU/dha' 142g 6 I W 1935 5 Sheets- Sheet 5 M. R. FENSKE ET AL Filed Nov. 21,

PROCESS FOR TREATING MINERAL OILS April 14, 1936.

5 i it t IE5 YHMHWW J Patented Apr. 14, 1936 PROCESS FOR TREATING-MINERAL OILS Merrell R. Fenslre and Wilbert B. McCluer, State College, Pa., assignors to Pennsylvania Peorporation, a corporation -troleum Research of Pennsylvania Application November 21, 1933, Serial No. 699,050

13 Claims. This invention pertains generally to the treatment of mineral oils and pertains particularly to the solvent extraction and/or fractionation thereof.

In copending application, Serial No. 688,416 by Merrell R. Fenske and Wilbert B. McCluer, is described a process and apparatus for the extraction and/or fractionation of mineral oils wherein a plurality of liquids of different densities are flowed countercurrently to each other by virtue of differences in their densities. The types of apparatus described in said copendingapplication employ columns of the order of distillation or fractionation columns. In practicing said invention, the liquids enter the column at points which skilled in the art as the specification proceeds and upon reference to the drawings in which ,llike reference characters have been appended to are spaced vertically along said column. At leastone light solution of the liquids is taken off from the column at the top thereof, and at least one heavy solution of the liquids is taken off from the column at the bottom thereof.

The liquids employed in said process generally comprise a mineral oil and a solvent or solvents. If more than one solvent is employed the solvents may be mixed prior to their introduction into the column or one or more of the solvents may be mixed with the oil prior to its introduction into the column, or one or more of the solvents may be fed into the column at aseparate point or points.

The invention herein comprises a specific form' oi the process and apparatus of the said copending application. It is specifically adapted for the Etreatment of -a mineral oil with two or more solvents of different densities. It is particularly applicable when one solvent is lighter than the ,oil and another solvent is heavier than the oil,

'ai'though this is by no means an essential feature as will .hereinafter. appear.

The liquids enter the column at vertically spaced points. For instance, a heavy solvent may enter the column at a high point, a light solvent may enter the column at a low point and an oil may enter the column at an intermediate point. By this means the oil and two solvents are caused to flow counter-currently to each other through the column and are brought into intimate contact therein to form two or more countercurrently flowing solutions of difierent densities which are taken oil at the top and bottom of said column.

Other features of the invention reside in the construction, arrangement, and combination of parts, and in the steps, combinations and sequences of steps, all of which together with other features will become more apparent to persons like parts in the various figures, and in which:

Figure 1 is an elevation of a column of this invention.

Figure 2 is a sectional elevation of the column of Figure 1.

Figure 3 is a section on line 3-3 of Figure 2.

Figure 4 is a section on line 4-4 of Figure 2.

Figure 5 is a section on line 5-5 of Figure 2.

Figures 6a and 6b comprise a broken sectional elevation of another formof the invention. Figure 7 is' a section on line 1-1 of Figure 6a..

Figure 8 is a section on line 8-8 of Figure 6a. Figure 9 is asectional elevation of a further form of the invention.

Figure 10 is a section on line lfl-IO of Figure 9..

Figures 11a and 11b comprise a broken section of the further form of the invention.

Referring now more particularly to Figures 1 to 5 inclusive, at III is shown a column comprising an upper portion II and a lower portion I 2. Section I I at its upper end is connected to a solution segregating chamber l3 as by flanges illustrated at 14. segregating chamber I3 is connected at its upper end to a feeding chamber is. The connection is illustrated as being made by flanges l6.

One of the flanges I6 is illustrated as being integral with a plate I! which extends across the lower end of feeding chamber' l5. Plate ll is provided with a plurality of apertures i8 in which are secured the upper ends of feeding tubes 19.

Section i I at its lower end is connected to the upper end of feeding chamber 2 l The connection is illustrated as being made by flanges 22 and 23. Flange 22 is illustrated as being integral with a plate 24 which extends across the lower end of shell 25 of section II.

The lower fiange at I4 is illustrated as being integral with a plate 26 which extends over the upper end of shell 25 of section r Plates 24 and 26 have a plurality of apertures 28 and 29 respectively which are aligned with eachother and receive the opposite ends of a plurality of tubes 30 of substantially equal diameter and length. Tubes 30 may, if desired, be

. the means illustrated at 32.

Packing 3| may be of any suitable character. 66

ployed. However, a packing which is. particularly emcient is one which aifords-"a' relatively high surface area with arelativelyhig'h percentage of free space. '11ie efficiency of the solvents is greatly increased thereby. Such packing is more particularly described in said copending application and in copendi'ng application Serial No.

877,755 flied June 26, 1938. This ty es! packing has many forms of which carding teeth, single turn, double turn, triple turn or polyturn helixes, open rings, bent carding teeth, H-shaped, 8- shaped, and #-shaped wire forms are representative. The size of the wire may be comparable to that ofordinary carding teeth used in the textile industry and the dimensions of the various forms may also be generally comparable thereto. Other sizes may be employed.

Each tube II is associated with a separate tube II and extends downwardly therein as illustrated.

Lower section I! as illustrated is identical with upper section I i and corresponds to the inversionof upper section II.

Section II has a shell 34 which at its upper end is joined to the lower end of feeding chamber II as by flanges 85.

a plate It whichextends over the ,upper end of shell 34.

Shell 34 at its lower end is Joined to the upper end of segregating chamber II as by flanges ll. The upper of the two flanges 39 is illustrated as being integral-with plate 40' which extends over the lower end of shell as. Plates I6 and 40 have a plurality of apertures ll and 42 respectively, which are aligned so as to receive a plurality of uibes 43 of substantially equal diameter and length.

Tubes 48 are shown packed with a packing All, which may be supported in each tube by any suitable means such as the device 45 illustrated at the lower end thereof. Packing 44 may correspond to packing II.

segregating chamber 3| at its lower end is connectedto feeding chamber 48 as by flanges 41.

One of the flanges 41 is illustrated as being integral with a plate ll which extends over the upper end of feeding chamber ll. Plate 4! is a duplicate of plate I! and is provided with a plurality of apertures u in which are ,fltted feeding tubes ll.

Each tube It is associatedwith a separate tube It and extends upwardly therein for feeding purposes.

Chamber II is illustrated as having an inlet I2 controlled by a valve 53 chamber I3 is illustrated as having an outlet 54 controlled by a valve I;

chamber II is illustrated as having an inlet I. controlled by a valve 51; chamber 38 is illustrated as having an outlet 58 controlled by a valve 59; and chamber 48 is illustrated as having an inlet ll controlled by a valve 8|.

. Inlet It is shown connected to a liquid distributor I which may be of any suitable type.

Distributor .3 as shown comprises extensions 84 The lower of the two flanges ii is illustrated 'as being integral with I Any of the various packings employed in distil--- lation and fractionation processes may be. ernthrough tubes II into tubes ll. If tubes II are of substantially equal diameter and len th. the heavy solvent will be substantially equally distributed between the tubes Ill.

Light solvent is similarly fed in at ll into chamber 8 from which it flows through tubes I. up into tubes ll. The light solvent will be substantially equally distributed between tubes 48 if tubes ID are of substantially equal diameter and length.

Oil is fed at it into chamber 2| and then through the distributor OI. If annular spaces it are of substantially equal cross-section and length the oil will'be fed uniformly into each path formed by each aligned pair of tubes II and 43. It will be understood that other metering means may be provided in place of tubes It, or ll. or in place of distributor S3.

The down flowing heavy solvent and the up flowing light solvent contact the oil and each other. The oil tends to'rlse in the heavy solvent and to fall in the light solvent. The light solvent rises in the heavy solvent. If all three liquids are partially miscible in each other, the result will be the formation of at least two tertiary solutions of different densities. The light solution flows upwardly in view of the greater density of the heavy solvent and heavy solution. The heavy solution flows downwardly. The up flowing liquids come in contact with the down flowing fresh heavy solvent, and the down flowing liquids come in contact with the up flowing light solvent, the result of which is 'that by the time the lighter materials reach chamber II substantially nothing is present but light solution and by the time the heavier materials reach chamber 38 substantially nothing is present but heavy-solution. The light solution segregates itself in chamber it and the heavy solution segregates itself in chamber 3!.

A countercurrent extraction and/or'fractionation system is thus provided in which two or more solvents flow countercurrently .to each other, in which the mineral oil to be extracted and/or fractionated is introduced into said countercurrentlyflowing solvents at a point in the common path thereof, and in which said liquids contact each other substantially uniformly over .a relatively large surface area.

It causesthe liquids to spread out into fllms of relatively large surface area compared to their volumes. The effect is greater when the more efllcient packing materials are employed such for instance as those specifically described v herein.

The tubes ll and 43 may have a cross section of any desired geometrical conflguration and within certain limits of any desired area. The cross section of each tube is preferably limited to an area sufllclently small to prevent serious channeling after any contacting means, for instance packing, has been arranged therein. The preferred limiting cross sectional area for each tube will be not only a function of the type of contacting means employed, since the small wire forms described-herein will as a rule permit the use of a larger cross section without an inordinate falling off of efficiency than raschig rings or jack chain, but also of the manner in which the contacting means is arranged in each tube, for instance, of the degree of uniformity of distribution of packing. Since the tubes may hm sides which are mam crummother surfaceconilgimflon. the

' tial increase in efficiency which we have dispressure and normal temperatures, or by both.

' should this be desirable for any reason, for inwith a plurality'oi' openings ll.

covered results from a. constriction ofcross sectional area cannot be given but may be readily determined, for instance, by testing the efficiency of single tubes ofzdifferent sizes after any contacting means to be employed is arranged therein.

It may be stated as a general rule that one should proceed with caution after exceeding a cross sectional area equivalent to that of a circular tube in the neighborhood of three inches in diameter although, with the proper selection of packing or other contacting means and a careful distribution in each tube, it is possible that larger cross sectional areas may be employed while in other cases smaller cross sectional areas may be Therefore, the term 'frelatively small,

cross sectional area" or its equivalent when employed in this specification andin the claims is intended to meana cross section which, when taken in conjunction with any contacting means, issudiciently small to materially increase the contacting efficiency because of the constriction of its area.

Each solution will contain oil and solvents in different proportions. The solvent maybe removed from each 011 portion by any suitable means, for instance, by distillation if the solution is a liquid at room temperatiires and atmospheric pressure, or by reducing the pressure if the solvent employed is a vapor at atmospheric If the process is carried out .for the purpou of extraction, one of the oil portions will comprise ramnate and the other extract. If the process is carried out for the purpose of fractionation, one of the all portions will have a greater viscosity than the other or in other words each portion will comprise a different fraction.

Thecolumn may be operated at any desired pressure. This pressure may be atmospheric, particularly if the solvents are liquid at atmospherlc pressure, or elevated, particularly if this is necessary to maintain one or more of the solvents in the liquid phase (partially or wholly, as desired) while in the column, or reduced,

stance, 'to bring a part of the solvent or solvents into the vapor phase.

The feeding rate of each solvent and of the oil should be such as to permit the countercurrent flow above referred to. The desired heavy. solvent to light solvent ratio and the desired heavy solvent and/or light solvent to oil ratios will, .of course, determine the relative rates of feeding of the solvents and of the oil.

In order to facilitate segregation at the bottom of the column and to assist the countercurrent now, the segregated heavier solution is preferably maintained at a suitable level in chamber 88 above the outlet 58.

Shell 25 is shown provided with a plurality of openings 10 and shell is shown provided Openings in and II are provided for. the purpose of circulating a heating or cooling fluid such as water,

steam or brine about tubes SI and 43 respec tlvely for temperature controrpurposes.

Tubes 30 and I may be of any desired number, that is, one or more. The number employed will eczema f overmd by the desired m'.

an effort should be made to pack eachsetoftubeslland-lluniformlyorsimi-' larly so that the pressure drop-through each tube of each set will be substantially the same."

Substantially the same conditions will then uist in eachtube of each set. Uniformityof resultsin eachtube ofeachsetisthus-assm'ed.

Since the'resultof having the tubesof subsubstantially stsntially the same size and of equally dividing. each feed liquid among the tubes is to maintain substantially the same ofeachphasetotheothersineachtubeit [be obvious that the'tubes may beef diiferen sizes and that the feeding-rates may vary-ac cordingly particularly if substantially the same proportion of phases is maintained in each tube.

In other words, the result of having the .ofthe same size and of maintaining unif feeding conditions ineach tube is to cause rafilnate phase produced by each tube to substantially the same eompodtion as "'nate phase produced by any other tube and to cause the extract phase produced by any: tube to be of substantially the same .composition the extract phase produced by any other tube. From this it will be obvious-that ifthe tubes 1 should vary in size the feeding; rates may be adiusted to obtain'simiiar conditions.

The column may have-any height selected will be somewhat governed by the eiiiciency of the contact mechanism employed,

and the desired time of contact between each unit volume of one'liquid with any of the other" liquids. c Thecolumns'howninl iguresltobinclusive is highly efficient and useful for the purposes for which it is intended. The llqtildfflOW there-' through in a plurality of streams of substantially equal size without serious channeling particularly if the tubes are of relatively small dimeter and substantially uniformly packed. It is to be understood that in its broader phases the invention includes other forms.

A different column, for instance, is

at It in Figures 6ato8 inclusive. Column It can-- prises an upper portion II and a lower portion 16. Upper portion 15 is joined at its upperend to the lower end of feeding and segregating chamber ll as by flanges 18 and I8.

Flange" is illustrated as being integral with a perforated plate which extends across the upper end of shell ll of portion II. V a

Portion ll is illustrated as being connected at its lower end to the upper end of feeding champroportion' will , 30 desired height. The

bers "may be of any desired character and preferably have relatively large surface areas. Jack, chain or a similar material may be employed for this purpose. Feeding chamber I! is connected at its lower end to the upper end of portion" as by flanges l0 and ll. Flange Ii is illustrawd as being'integral witb--a-..plate"l2 which extendsacross the upper endof shell as of portion It.

The lower end'of portion 1! is joined. to the upper end of feeding and segregating chamber stasbyilangesllandit-Flangellisilltl- 1s trated as being integral with a perforated plate 01 which extends across the lower end of shell 00 of portion 10.

A plurality of attenuated members 00 extend between plates 02 and 01 and are secured thereto as by eye bolts 00 and I00 respectively.

An. inlet is illustrated at I02. Another inlet is illustrated at I00, and a third inlet is illustrated at I04. The inlets I02, I00, and I04 are illustrated as being connected to liquid distributors I00, I00, and I01 respectively.

Chamber 11 is illustrated as having an outlet I00 at its top which leads to a receiver I00. Chamber 04 is illustrated as having outlet H0 at its bottom which leads to a receiver III.

From the foregoing it will be obvious that attenuated members 00 and 00 might be Joined across chamber 02 or its equivalent with or with= out the use of plates 00 and 02 thus substituting each aligned pair of attenuated members 00 and 00 with a single attenuated member.

One manner of operation is as follows. .Heavy solvent is fed at I02, oil is fed at I00 and light solvent is fed at I04. Each flows through the column 14 in the manner previously described in connection with the form shown in Figures l to 5. The result; is the formation of two tertiary solutions. One solution flows upwardly into chamber 11 where it becomes segregated from the heavy downwardly flowing solvent entering at I02, and flows out through outlet I00 into the receiver I00. The other solution flows downwardly into chamber 04 where it becomes segregated from the light upwardly flowing solvent entering at I04, and flows out through outlet I I0 into the receiver III.

The segregated heavy solution is preferably maintained at a suitable level in chamber 04 to facilitate its segregation and to improve the operatlon of the column.

The attenuated members 00 and 00 cause the liquids to spread out into thin films, and to flow through the devious paths thus causing them to intimately contact each other. Members 00 and 00 may be of any desired number and are preferably closely spaced. The number shown in the drawings is not intended to be representative.

This form of the invention may also be provided with heat exchange means, for instance, by providing the shells 0I and 00 with Jackets for the flow of either a heating or a cooling fluid. Such jackets are illustrated at H2 and H0.

A further form of apparatus is illustrated in Figures 9 and 10. In this form column IIO comprises upper portion H0 and lower portion II1. Portion I I0 at its upper end connects to a feeding and segregating chamber I I0 as by flanges H0 and I20.

Flange H0 is illustrated as being integral with a perforated plate I2I which extends across the upper end of shell I22 of portion I I0.

Portion IIO is illustrated as being connected at its lower end to the upper end of feeding chamber I23 as by flanges I24 and I20. Feeding chamber I23 is illustrated as being connected at its lower end to the upper end of portion II1 as by flanges I20 and I21.

The lower end of portion I I1 is illustrated as being connected to the upper end of feeding and segregating chamber I20 as by flanges I20 and I00.

Flange I30 is illustrated as being integral with a perforated plate IOI. Perforated plates I2I and IN support therebetween a plurality of attenuated members I00 which are illustrated as being discontinuous at chamber I23 although they may be continuous as will be obvious. Each attenuated member I00 comprises a rod I04 having a plurality of spaced discs I05. Discs I00 on ad- Jacent rods are preferably vertically spaced from each other and preferably overlap laterally as i1- lustrated. Any suitable order for the discs I00 may be chosen, for instance, that illustrated, having in mind the purpose thereof.

Inlets I31, I00, and I00 are illustrated as being connected to distributors I40, I, and I42 respectively.

Chamber H0 is illustrated as having outlet I44 at its top which leads to a receiver I40.

Chamber I20 is shown with an outlet I40 at its bottom which leads to a receiver I 41.

Any type of temperature control means such as Jackets for steam, water or brine may be provided for controlling the temperature of the liquids while in the column.

The feeding of liquids into column IIO may be similar to that described in connection with the previous forms in which case the heavy solvent, oil, light solvent, heavy solution and light solution will be brought into intimate contact as they pass through the devious paths provided in the column'by the attenuated members I30. Members I00 may be of any desired number.

.Many other variations in constructional form may be resorted to.

The solvents may comprise a single or a plurality of compounds. When a plurality of compounds are employed, they may be miscible or partially miscible. A plurality of non-miscible solvents might also be employed.

In the apparatus previously described when the result is the formation of two non-miscible solutions of different density, one of the solutions will be segregated and taken oif at the top of the column and the other will be segregated and taken off at the bottom of the column. Should the result be the formation of more than two non-miscible solutions such as three, the third solution will rise with the lightest solution or will settle with the heaviest solution, depending among other things on the relative densities of the solutions and the rates and points of feed of the various liquids into the column.

The third solution may be removed from the column along with the lightest solution or along with the heaviest solution as the case may be, and the twosolutions may be separated by any suitable means such as by decantation.

However, the segregating chambers at the top and bottom of the column may be so constructed as to continuously segregate the two solutions. This is illustrated in Figures 11a and 11b in which Figures 2a and 2b have been substantially reproduced except that tubes 3 la extend up into chamber I3 to a point substantially midway thereof; tubes 40a extend downwardly into chamber 00 to a point substantially midway thereof; outlet 04 of chamber I0 has been substituted by outlets I00 and I 0| at the top and bottom of chamber I3; and outlet 00 of chamber 00 has been substituted by outlets I02 and I00 at the top and bottom of chamber 00.

The operation of the invention illustrated in Figures 11a and 11b is as follows: Let it be assumed that two of the three or more non-miscible solutions rise in the column. These two solutions will be delivered to chamber I 0 through tubes 0 In. The two solutions separate due to differences in density and the lighter solution is taken oi! at I 00 a,osv,s1o 5 and the heavier solution at Ill. The W of extending tubes flu is to deliver the two solutions tothe chamber I! at a point at which the concentrations of the solutions in chamber'll are substantially the same as their concentrations when they leave the tubes ila.

Should the two solutions settle in the column,

the lighter of the two would be withdrawn at III and the heavier at I53.

The modified construction of Figures 1111 and 11b would take care of a 4 layer system if the column were operated so that two of the nonmiscible solutions would rise and the other two would settle. However, the construction might be modified to takecare of three or more non-miscible layers in one segregating chamber if such conditions were obtained. Y

It is to be particularly noted that the construction of Figures 110 and 11b would separate any non-miscible liquids which might reach the segregating chambers regardless of whether two or more solutions were formed.

While the invention has been particularly described in connection with the treatment of mineral oils, it may also be applied to'the treatment of materials in general, whether or not the more valuable, the less valuable, or an equally voluable material is separated from the base material. While in the foregoing description the solvents have been referred to as being fed into the column at the ends thereof and the oil as being fed into the column at an intermediate point, this is by no means an essential feature. Any one or more of the liquids might be fed into the column at an" intermediate point or points if desired for any reason, or certain of these liquids might be fed in at the ends while one or more of the liquids are fed into the column at an intermediate point or points. In general, the liquids will'be fed into the column at vertically spaced points in the order of their densities, the density increasing from thebottomtothe top. Thisrule may be departed from but in any case, the densi-. ties of the respective liquids and the densities of the solutions formed will be taken into considera- 7 tion.

For instance. the oil might be fed in at the top of the column, one solvent at an intermediate point, and a second solvent at the bottom. particularly in cases in which the'oil is heavier than the solvents. Or, in the latter case, the oil might be fed in at an intermediate point, the lighter solvent at the bottom, and the heavier solvent at the top, particularly .if the heavier solvent is heavier than the light solution.

The oil might fed in at the bottom, one solvent at an inte ediate point, and another solvent at the top, particularly when the oil is lighter than both solvents. In the latter case the lighter of the solvents could be fed in at the bottom, the oil at an intermediate point, and the heavier solvent at the top, particularly if the lighter solvent is lighter than the heavier solution.

In cases in which the oil is fed either at the top or at the bottom and both solvents flowcountercurrently to the oil, the. oil meets two different solvent conditions in the column. For

instance, in cases in which the oil is introduced at the top of the column and flows downwardly and the two solvents flow upwardly, the oil is first treated by a mixture of the two solvents and 1 then after it passes the intermediate point of solvent feed, it is treated by one solvent alone.

- The same is true when the oil is fed at the botbecoming familiar herewith.

tom of the column and both solvents fiow countercurrently thereto.

, The solvent introduced at the intermediate point may or may not cause precipitation of the material and/or may or may not be selective as .to the same type and/or size of molecule obtained with the oil entering at an intermediate point, if one solvent were selective as to one type of molecule and the other as to another type of molecule, one of the solutions which is taken Loif at one end would have a preponderance of one .type of molecule and the other solution taken n at the opposite end of the column would have a preponderance of another type of molecule.

Other methods of feeding the column will suggest themselves to persons skilled in the art upon The following specific examples will serve to further illustrate the foregoing.

For instance, pyridine which has a density of .99 can be fed at the top, methylcellosolve which has a density of .96, or methanol which has a density of .8, or both can be fed at the bottom and oil of any density, say, for instance, .92, can

be'fed at an intermediate point. Or the feeding points of oiland methylcellosolve may be hydrlc aliphatic alcohol at an intermediate and acetone at the bottom. Other combinations will suggest themselves to persons skilled in the. art upon becoming familiar herewith.

Any of the columns may be operated at elevated pressures, atmospheric pressure, or reduced pressures as previously referred to.

- reversed. Or oil can be fed at the top, a mono- The term solvent in its broader phases in- 1 eludes any compoimd or compounds, whether in I the. vapor, liquid and/or solid phase and regardless of its infiuenceupon the Although the liquids have been referred .to as being partially miscible, it.- is to be keptin mind that miscibility is a function of temperature and relative concentrations. It would, therefore. be possible to raise the temperature of the liquids in the column so as to cause complete solution of two or more or all of the liquids therein, in which case separation might be eflected upon cooling of the solution or solutionsthus obtained.

The relative densitiesof solvents and'of mineral oils may be obtained upon reference to any standard handbook or by actual ent.

Particular forms of apparatus have been described for the purpose of illustration. It is to be strictly understood that'wide departures may be I therefore, are intended to be limited only as required by the prior art.

' The term phase terms as used lngthe claims denotes a'patl! adapted intimately contact oi mix l q d phases passing therethrough as distinguished from channeling caused by phase separation.

The terms substantially equal, substantially the same and similar terms as used herein have a sufliciently broad significance to include equal, the same, etc.

The term vertically arranged" as used in the specification and in the claims to describe the positioning of the attenuated packing members includes not only an arrangement wherein the attenuated packing members are positioned perpendicularly to the plane of the horizon but also an arrangement wherein the attenuated packing members are sufficiently upright to carry out the purposes of this invention.

Reference is made to copending applications Serial No. 10,932 filed March 13, 1935, Serial No. 704,052 filed December 26, 1933, and Serial No. 708,515 filed January 26, 1934.

We claim:

1. A process for contacting at least three liquid phases of incomplete and partial miscibility to form at least two resultant phases such as in the solvent treatment of mineral oils, comprising introducing said initial phases. into a plurality of phase contacting paths connected in parallel, arranging the points of introduction of said initial phases into said phase contacting paths such that at least two of said initial phases will fiow countercurrently to each other in said phase contacting paths by virtue of a difference in their densities, and confining each phase, contacting path to a relatively small cross sectional area so as to prevent substantial channeling 01' said phases through each other.

2. A process for contacting at least three liquid phases of incomplete and partial miscibility to form at least two resultant phases such as in the solvent treatment oi! mineral oils, comprising introducing said initial phases in substantially the same proportions one to the other into a plurality of phase contacting paths connected in parallel, arranging the points of introduction of said initial phases into said phase contacting paths such that at least two of said initial phases will fiow countercurrently to each other in said phase contacting paths by virtue of a difference in their densities, and confining each phase contacting path to a relatively small cross sectional area so as to prevent substantial channeling of said phases through each other.

3. A process for contacting at least three liquid phases of incomplete and partial miscibility to form at least two resultant phases such as in the solvent treatment of mineral oils, comprising introducing said initial phases in substantially the same proportions one to the other into a plurality of phase contacting paths, arranging the points of introduction of said initial phases into said phase contacting paths such that at least two of said initial phases will flow countercurrently to each other in said phase contacting paths by virtue of a difference in their densities, confining each phase contacting path to a relatively small cross sectional area so as to prevent substantial channeling of said phases through each other, removing and uniting the streams of the lighter of said resultant phases at the tops of said. phase contacting paths, and removing and uniting the streams of the heavier of said resultant phases at the'bottoms of said phase contacting paths.

4. In a proces for contacting a mineral oil and at least two solvents wherein at least two of said liquids are caused to flow countercurrently to each other by virtue of a difference in density, I the steps of dividing each of said liquids into a plurality of relatively small streams, contacting said streams so that each stream of each liquid contacts one stream of each of the other liquids in an elongated phase contacting path which is segregated from all of the other streams, at least three of said liquids having each a. separate point of entry into said paths, and substantially uniformly distributing the counterfiowing streamsacross the cross section of each phase contacting path by confining each phase contacting path to a suiilciently small cross sectional area.

5. In a process for contacting a mineral oil and at least two solvents wherein at least two of said liquids are caused to flow countercurrently to each other by virtue of a difference in density, the steps of dividing each of said liquids into a plurality of relatively small streams, contacting said streams so that each stream of each liquid contacts one stream of each of the other liquids in an elongated phase contacting path which is segregated from all of the other streams, substantially uniformly distributing the counterflowing streams across the cross section of each phase contacting path by confining each phase contacting path to a sumciently small cross sectional area to prevent serious channeling, and introducing said liquids into each phase contacting path in substantially the said proportions one to the other.

6. In a process for contacting a mineral oil and at least two solvents wherein at least two of said liquids are caused to flow countercurrently to each other by virtue of a difference in density, the steps of dividing each of said liquids into a plurality of relatively small streams, contacting said streams so that each stream of each liquid contacts one stream of each of the other liquids in an elongated phase contacting path which is segregated from all of the other streams, substantially uniformly distributing a packing medium in each phase contacting path, and confining each phase contacting path to a suificiently small cross sectional area to prevent serious channeling.

7. In a process for contacting a mineral oil and at least two solvents wherein at least two 01' said liquids are caused to flow countercurrently to each other by virtue of a diil'erence in density, the steps of dividing each liquid into -a plurality oi. relatively small streams, contacting said streams so that each stream of each liquid contacts one stream or each 01' the other liquids in an elongated phase contacting path which is segregated from all 01' the other streams, substantially uniformly distributing the counterfiowing streams across the cross section of each phase contacting path by confining each path to a sufilciently small cross sectional area to prevent serious channeling, and combining the streams oi. each resultant phase after leaving said phase contacting paths.

8. A process for contacting an oil and a plurality of solvents, comprising introducing said liquids at three vertically spaced points into a column having a plurality oi attenuated packing members vertically arranged therein, said packing members being spaced from each other, and choosing the points of introduction 01' said liquids into said column such that at least two 01 said liquids will flow through said column countercurrently to each other.

9. In a process involving the contacting of a mineral oil and at least two solvents in a common path wherein at least two of said liquids are caused to flow countercurrently to each other by virtue of a difference in their densities, the steps of causing at least one of said liquids to flow through said common path in a widely distributed form by conducting said liquid through said common path over a plurality of vertically arranged packing mediums each of which has a relatively long and narrow shape, said packing mediums being wetted by said liquid.

10. In a process involving the contacting of a mineral oil and at least two solvents in a common path wherein at least two of said liquids are caused to flow countercurrently to each other by virtue of a difference in their densities, the steps of causing at least one of said liquids to flow through said common path in widely distributed form by conducting said liquid through said common path over a plurality of vertically arranged packing mediums each of which has a relatively long and narrow shape, said packing mediums being wetted by said liquid, and separately encasing each'oi said packing mediums to confine said counterfiow to said packing mediums.

11. A process for treating a mineral oil with a plurality of solvents, comprising introducing said liquids into a contacting column at vertically spaced points, said column comprising a group of phase contacting paths of relatively small cross sectional area and connected in parallel, the points of entry oi. said solvents into said parallelly connected phase contacting paths being spaced from each other and from the point or entry of said 011, said points of entry of said solvents being on the same side of the point of entry of said oil, and choosingsaid solvents as to density so that said solvents will flow through said column in the same direction and countercurrently to said oil.

said solvents will flow through said column in opposite directions, and confining each phase contacting path to a suflloiently small cross sectional area to prevent substantial channeling.

13. A process for contacting at least three liquid phases of incomplete and partial miscibility to form at least two resultant phases such as in the solvent treatment of mineral oils, comprising introducing said liquids at three vertically spaced points into a column having a plurality of attenuated packing members vertically arranged side by side therein, said packing members having spaces therebetween, and choosing the points of introduction of said liquids into said column such that a least two of said liquids will .flow through said column countercurrently to each other.

. MERRELL R. FENSKE.

WILBERT B. McCLUER.' 

